CN102977838A - Moisturecuring polyurethane hot melt adhesive for lining cloth and preparation method of moisturecuring polyurethane hot melt adhesive - Google Patents
Moisturecuring polyurethane hot melt adhesive for lining cloth and preparation method of moisturecuring polyurethane hot melt adhesive Download PDFInfo
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Abstract
The invention discloses a moisturecuring polyurethane hot melt adhesive for lining cloth and a preparation method of the moisturecuring polyurethane hot melt adhesive. The preparation method comprises the following steps of: 1, heating and melting polyester polyol, polyether polyol, antioxidant and tackifying resin, stirring and mixing uniformly, and vacuum-degassing for 3.0h; 2, under the protection of nitrogen, adding MDI (diphenyl-methane-diisocyanate) and a catalyst in the reaction system, reacting for 45min at a temperature of 85-95 DEG C; 3, under the protection of nitrogen, adding a chain extender, a silane coupling agent and nanoscale white carbon black, reacting for 1.0h at a temperature of 85-95 DEG C to obtain a prepolymer; and 4, under the protection of nitrogen, transferring the reaction mixture to an aluminum foil bag, sealing and then curing for 6h at a temperature of 85 DEG C to obtain the moisturecuring polyurethane hot melt adhesive with wide and adjustable coating temperature and little residual CO2. The moisturecuring polyurethane hot melt adhesive is especially suitable for the industry of the lining cloth, and has the characteristics of high stripping strength and wide and adjustable sizing temperature.
Description
Technical field
The present invention relates to a kind of lining cloth with moisture-curable polyurethane hot melt adhesive and preparation method thereof, belong to the polyurethane adhesive synthesis technical field.
Background technology
Moisture cure urethanes adhesive is a kind of novel tackiness agent, its tackiness agent mechanism is different from the gluing mechanism of other tackiness agent, hydrogen bond in traditional tackiness agent is not only arranged, the realizations such as Intermolecular Forces and base material bonding, and meanwhile wherein-the NCO group be diffused into the reaction of moisture of colloid inside, generated the amino that contains reactive hydrogen, then producing urea groups with-NCO radical reaction, and then the formation crosslinking structure, realize solidifying.Not only again melting of colloid after solidifying, and owing to the active component in the colloid and the corresponding active component reaction in the base material, greatly strengthened the bonding strength of glue.Standard of living raising along with people, requirement and demand for the Clothing Consuming product are more and more higher, the fabric lining cloth of various specific function materials is compound more and more, the material of various fabrics, quality difference, and the type of the tackiness agent of required usefulness and applying glue temperature are also different.Numerous research staff have developed and have been permitted eurypalynous hot melt adhesive, but every kind of colloid is all because some defective of self, and can not comprehensively satisfy lining cloth industrial development requirement.The development and application of moisture cure urethanes adhesive, because its excellent over-all properties, that uses in the fabric composite industrial is more and more extensive, the present invention focuses on the high-performance hot melt adhesive that each temperature range of research and development is used, pass through its reasonable modification simultaneously, under the prerequisite that guarantees its performance requriements, reduce its production cost.
Summary of the invention
The present invention seeks in order to overcome the deficiency of prior art, for the preparation of multifunctional polyurethane hot melt adhesive provides new synthetic method, product is mainly used in lining cloth industry poly fleece, four sides elasticity cloth, diablement fort and to functional membranes such as waterproof, anti-electrostatic, waterproof ventilated membranes, the textiless such as shoes cap bonding.
The solution of the present invention is:
A kind of lining cloth moisture cure urethanes adhesive and preparation method thereof is characterized in that may further comprise the steps:
(1) with a certain amount of polyester polyol, polyether glycol, antioxidant, tackifying resin, mix 130～145 ℃ of lower heated and stirred, simultaneously vacuum-drying 3.0h cools to 90 ℃;
(2) under nitrogen protection, MDI and catalyzer are joined in the product of step (1), and at 85～95 ℃ of reaction 45min;
(3) under nitrogen protection, chainextender, silane coupling agent, nano-scale white carbon black are joined in the product of step (2), and at 85～95 ℃ of reaction 1.0h, obtain prepolymer;
(4) under nitrogen protection, the product of step (3) is transferred in the aluminium foil bag, 85 ℃ of lower slakings 6 hours, obtain product after the sealing;
The number-average molecular weight of described polyester polyol is 1250～2000, is selected from a kind of in polyethylene glycol adipate glycol, polyhexamethylene adipate glycol, polybutylene glyool adipate, poly terephthalic acid hexylene glycol esterdiol, polybutylene terephthalate glycol, the Poly(Trimethylene Terephthalate) glycol;
The number-average molecular weight of described polyether glycol is 1000～4000, is selected from polyoxypropyleneglycol, polyoxyethylene glycol, a kind of in PTMG, the polyoxytrimethylene copolymerization glycol; .
Described MDI is diphenylmethanediisocyanate, be selected from 4,4 '-among MDI, 2,4 '-MDI, 2,2 '-MDI more than one; Described catalyzer is stannous octoate/pair (2,2-morpholine ethyl) ether composite catalyst, and wherein the mass percent of two (2,2-morpholine ethyl) ethers is 30%50%; Described chainextender is selected from butyleneglycol, propylene glycol, 1,6-hexylene glycol, a kind of in the glycol ether;
Be 100 parts by mass fraction, the mass fraction of above-mentioned each component is respectively:
1 ~ 17 part of polyester polyol, 40 ~ 60 parts of polyether glycols, MDI17.5 ~ 19 part, 0.5 part of antioxidant, 0.05 part of catalyzer, 17 ~ 19 parts of tackifying resins, 0.5 ~ 2 part of chainextender, 1 ~ 2 part of silane coupling agent, 0.1 ~ 2 part of nano-scale white carbon black..
Described tackifying resin is selected from polystyrene, and the polyethylene vinyl acetate multipolymer is more than a kind of the reaching in the polyacrylic acid.
Described silane coupling agent is selected from γ aminopropyltriethoxy silane KH-550, γ-glycidyl ether oxygen propyl trimethoxy silicane KH-560, γ-(methacryloxypropyl) propyl trimethoxy silicane KH-570, a kind of among the gamma-amino propyl trimethoxy silicane KH-551.
Described antioxidant is the CHINOX1010/CHINOX1076 compound antioxidant, and both mass ratioes are 1:1.
Beneficial effect of the present invention: the moisture-curable polyurethane hot melt adhesive of the present invention's preparation not only has the bonding of hydrogen bond, Intermolecular Forces realization and base material in traditional tackiness agent, and when sizing agent and the curing of steam reaction post-crosslinking, has improved its cohesive strength.Improving the result that can reach by technology of the present invention is:
1. applying glue temperature is extensively adjustable, can obtain the arbitrary temp scope applying glue from room temperature to 120 ℃, to be applicable to various fabric optimal temperatures.
2. in the moisture curing reaction process, steam generates CO with the reaction of-NCO
2, at first solidify on the sizing agent surface, the inner CO that produces of colloid
2Remain in the colloid, so that in thicker glue-line, honeycomb-like pores occurs, the present invention is CO by adding a small amount of nano-scale white carbon black
2Diffusion provides passage, alleviates the honeycomb-like pores of gas-bearing formation, so that the performance of product is better.
Embodiment
The invention will be further described below by embodiment, and its purpose only is to understand better content of the present invention, and unrestricted protection scope of the present invention, wherein said molecular weight is number-average molecular weight.
Embodiment 1
Take by weighing molecular weight and be 2000 polyphenyl dioctyl phthalate butanediol ester glycol 5.0g, the polyoxypropyleneglycol 300.0g of molecular weight 4000, polyacrylic acid 85.0g, each 1.25g of antioxidant CHINOX1076 and CHINOX1010, add in the there-necked flask, heated and stirred, and under 130～145 ℃ of conditions vacuum 3.0h.Vacuum tightness is being lower than 0.1 normal atmosphere.Cool to 90 ℃, add 4,4 under the nitrogen protection '-MDI87.5g, stannous octoate 0.175g and two (2,2-morpholine ethyl) ether 0.075g, under 85 ~ 95 ℃ of conditions, reaction 45min.Under the nitrogen protection, add BDO 4.75g, γ aminopropyltriethoxy silane KH-55010.0g, nano-scale white carbon black 5.0g, 85 ~ 95 ℃ of lower high-speed stirring reaction 1.0h.In the nitrogen protection bottom discharge and pack, slaking is 6 hours in 85 ℃ of environment with above-mentioned performed polymer.Namely obtain lining cloth fabric composite gum, sample number into spectrum is PUR-1.
Embodiment 2
Take by weighing molecular weight and be 2000 polybutylene glyool adipate 85.0g, molecular weight is 2000 polyoxyethylene glycol 210.0g, polystyrene 94.25g, each 1.25g of antioxidant CHINOX1076 and CHINOX1010, add in the there-necked flask, heated and stirred, and under 130～145 ℃ of conditions vacuum 3.0h.Vacuum tightness is being lower than 0.1 normal atmosphere.Cool to 90 ℃, add 2,4 under the nitrogen protection '-MDI95.0g, stannous octoate 0.125g and two (2,2-morpholine ethyl) ether 0.125g, under 85 ~ 95 ℃ of conditions, reaction 45min.Under the nitrogen protection, add 1,3-PD 2.5g, γ-glycidyl ether oxygen propyl trimethoxy silicane KH-56010.0g, nano-scale white carbon black 0.5g, 85 ~ 95 ℃ of lower high-speed stirring reaction 1.0h.Above-mentioned performed polymer in the nitrogen protection bottom discharge, and is packed, and slaking is 6 hours in 85 ℃ of environment.Namely obtain lining cloth fabric composite gum, sample number into spectrum is PUR-2.
Embodiment 3
Take by weighing molecular weight and be 1250 polycaprolactone polyol 44.75g, molecular weight is 4000 polyoxypropyleneglycol 255.0g, polyethylene vinyl acetate multipolymer 95g, each 1.25g of antioxidant CHINOX1076 and CHINOX1010, add in the there-necked flask, heated and stirred, and under 130～145 ℃ of conditions vacuum 3.0h.Vacuum tightness is being lower than 0.1 normal atmosphere.Cool to 90 ℃, add 2,2 under the nitrogen protection '-MDI87.5g, stannous octoate 0.15g and two (2,2-morpholine ethyl) ether 0.1g, under 85 ~ 95 ℃ of conditions, reaction 45min.Under the nitrogen protection, add 1,6-hexylene glycol 5.0g, γ-(methacryloxypropyl) propyl trimethoxy silicane KH-5705.0g, nano-scale white carbon black 5.0g, 85 ~ 95 ℃ of lower high-speed stirring reaction 1.0h.With above-mentioned performed polymer in the nitrogen protection bottom discharge and pack slaking 6h in 85 ℃ of environment.Namely obtain lining cloth fabric composite gum, sample number into spectrum is PUR-3.
Embodiment 4
Take by weighing molecular weight and be 2000 polyhexamethylene adipate glycol 85.0g, molecular weight is 1000 PTMG 200.0g, polyacrylic acid 95.0g, each 1.25g of antioxidant CHINOX1076 and CHINOX1010, add in the there-necked flask, heated and stirred, and under 130～145 ℃ of conditions vacuum 3.0h, vacuum tightness is being lower than 0.1 normal atmosphere.Cool to 90 ℃, add 4,4 under the nitrogen protection '-MDI89.75g, stannous octoate 0.13 and two (2,2-morpholine ethyl) ether 0.12g, under 85 ~ 95 ℃ of conditions, reaction 45min.Under the nitrogen protection, add glycol ether 10.0g, gamma-amino propyl trimethoxy silicane KH-551 7.5g, nano-scale white carbon black 10.0g, 85 ~ 95 ℃ of lower high-speed stirring reaction 1.0h.With above-mentioned performed polymer in the nitrogen protection bottom discharge and pack slaking 6h in 85 ℃ of environment.Namely obtain lining cloth fabric composite gum, sample number into spectrum is PUR-4.
Sample test
Test phase is used for fabricbase with above-mentioned four kinds of synthetic glue samples respectively under differing temps compound, and selected fabricbase is woven dacron, poly fleece and TPU waterproof and breathable composite membrane.Guarantee that in test process spread, humidity and curing environment are all identical.
Concrete operations are woven dacron/woven dacron, poly fleece/poly fleece, woven dacron/TPU waterproof ventilated membrane, poly fleece, waterproof ventilated membrane.The gluing temperature is respectively: 25 ℃, 70 ℃ and 120 ℃, measure result such as following table by the stripping strength after said sample is solidified:
Show 1PUR-1 stripping strength to different fabrics under differing temps
Show 2PUR-2 stripping strength to different fabrics under differing temps
Show 3PUR-3 stripping strength to different fabrics under differing temps
Show 4PUR-4 stripping strength to different fabrics under differing temps
。
Claims (4)
1. a lining cloth is characterized in that may further comprise the steps with moisture cure urethanes adhesive and preparation method thereof:
(1) with a certain amount of polyester polyol, polyether glycol, antioxidant, tackifying resin, mix 130～145 ℃ of lower heated and stirred, simultaneously vacuum-drying 3.0h cools to 90 ℃;
(2) under nitrogen protection, MDI and catalyzer are joined in the product of step (1), and at 85～95 ℃ of reaction 45min;
(3) under nitrogen protection, chainextender, silane coupling agent, nano-scale white carbon black are joined in the product of step (2), and at 85～95 ℃ of reaction 1.0h, obtain prepolymer;
(4) under nitrogen protection, the product of step (3) is transferred in the aluminium foil bag, 85 ℃ of lower slakings 6 hours, obtain product after the sealing;
The number-average molecular weight of described polyester polyol is 1250～2000, is selected from a kind of in polyethylene glycol adipate glycol, polyhexamethylene adipate glycol, polybutylene glyool adipate, poly terephthalic acid hexylene glycol esterdiol, polybutylene terephthalate glycol, the Poly(Trimethylene Terephthalate) glycol;
The molecular weight of described polyether glycol is 1000～4000, is selected from polyoxypropyleneglycol, polyoxyethylene glycol, a kind of in PTMG, the propylene oxide copolymerization glycol; .
Described MDI is diphenylmethanediisocyanate, be selected from 4,4 '-among MDI, 2,4 '-MDI, 2,2 '-MDI more than one;
Described catalyzer is stannous octoate/pair (2,2-morpholine ethyl) ether composite catalyst, wherein two (2,2-morpholine ethyl) ethers
Mass percent be 30%～50%;
Described chainextender is selected from BDO, 1,3-PD, 1,6-hexylene glycol, a kind of in the glycol ether;
Be 100 parts by mass fraction, the mass fraction of above-mentioned each component is respectively:
1 ~ 17 part of polyester polyol, 40 ~ 60 parts of polyether glycols, MDI17.5 ~ 19 part, 0.5 part of antioxidant, 0.05 part of catalyzer, 17 ~ 19 parts of tackifying resins, 0.5 ~ 2 part of chainextender, 1 ~ 2 part of silane coupling agent, 0.1 ~ 2 part of nano-scale white carbon black..
2. method according to claim 1 is characterized in that described tackifying resin is selected from polystyrene, and the polyethylene vinyl acetate multipolymer is more than a kind of the reaching in the polyacrylic acid.
3. method according to claim 1, it is characterized in that described silane coupling agent is selected from γ aminopropyltriethoxy silane KH-550, γ-glycidyl ether oxygen propyl trimethoxy silicane KH-560, γ-(methacryloxypropyl) propyl trimethoxy silicane KH-570, a kind of among the gamma-amino propyl trimethoxy silicane KH-551.
4. method according to claim 1 is characterized in that described antioxidant is the CHINOX1010/CHINOX1076 compound antioxidant, and both mass ratioes are 1:1.
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Address after: Qiandeng Town Wenpu road Kunshan city Suzhou City, Jiangsu province 215341 No. 366 Applicant after: KUNSHAN TIANYANG HOT MELT ADHESIVE Co.,Ltd. Applicant after: EAST CHINA University OF SCIENCE AND TECHNOLOGY Applicant after: SHANGHAI TIANYANG HOT MELT ADHESIVE Co.,Ltd. Address before: Qiandeng Town Wenpu road Kunshan city Suzhou City, Jiangsu province 215341 No. 366 Applicant before: KUNSHAN TIANYANG HOT MELT ADHESIVE Co.,Ltd. Applicant before: EAST CHINA University OF SCIENCE AND TECHNOLOGY Applicant before: Shanghai Tianyang Hotmelt Adhesives Co.,Ltd. |
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Address after: 215341 No. 366, Shipu Zhongjie Road, Qiandeng Town, Kunshan City, Suzhou City, Jiangsu Province Patentee after: Kunshan Tianyang New Material Co.,Ltd. Patentee after: EAST CHINA University OF SCIENCE AND TECHNOLOGY Patentee after: SHANGHAI TIANYANG HOT MELT ADHESIVE Co.,Ltd. Address before: 215341 No. 366, Wenpu Road, Qiandeng Town, Kunshan City, Suzhou City, Jiangsu Province Patentee before: KUNSHAN TIANYANG HOT MELT ADHESIVE Co.,Ltd. Patentee before: EAST CHINA University OF SCIENCE AND TECHNOLOGY Patentee before: SHANGHAI TIANYANG HOT MELT ADHESIVE Co.,Ltd. |
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Address after: 215341 No. 366, Shipu Zhongjie Road, Qiandeng Town, Kunshan City, Suzhou City, Jiangsu Province Patentee after: Kunshan Tianyang New Material Co.,Ltd. Patentee after: EAST CHINA University OF SCIENCE AND TECHNOLOGY Patentee after: Tianyang New Material (Shanghai) Technology Co.,Ltd. Address before: 215341 No. 366, Shipu Zhongjie Road, Qiandeng Town, Kunshan City, Suzhou City, Jiangsu Province Patentee before: Kunshan Tianyang New Material Co.,Ltd. Patentee before: EAST CHINA University OF SCIENCE AND TECHNOLOGY Patentee before: SHANGHAI TIANYANG HOT MELT ADHESIVE Co.,Ltd. |